朱世杰,王剑锋,刘欣玉,王利国,任晨星,常蕾,王俊,关绍康.可降解镁合金骨螺钉表面微弧电泳水热复合涂层的制备与性能[J].表面技术,2017,46(3):20-27.
ZHU Shi-jie,WANG Jian-feng,LIU Xin-yu,WANG Li-guo,REN Chen-xing,CHANG Lei,WANG Jun,GUAN Shao-kang.Preparation and Properties of Composite Coating by Micro-Arc Electrodeposition and Hydrothermal Synthesis on Surface of Biodegradable Magnesium Bone Screws[J].Surface Technology,2017,46(3):20-27 |
| 可降解镁合金骨螺钉表面微弧电泳水热复合涂层的制备与性能 |
| Preparation and Properties of Composite Coating by Micro-Arc Electrodeposition and Hydrothermal Synthesis on Surface of Biodegradable Magnesium Bone Screws |
| 投稿时间：2016-11-27 修订日期：2017-03-20 |
| DOI：10.16490/j.cnki.issn.1001-3660.2017.03.003 |
| 中文关键词: 生物镁合金 骨螺钉 电解抛光 微弧电泳 水热合成 复合涂层 羟基磷灰石 |
| 英文关键词:biomagnesium alloy bone screws electrolytic polishing micro-arc electrophoresis hydrothermal synthesis composite coating hydroxyapatite |
| 基金项目:“863”计划（2015AA033603, 2015AA020301）；河南省重大科技专项（141100310900） |
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| Author | Institution |
| ZHU Shi-jie | School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450001, China |
| WANG Jian-feng | School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450001, China |
| LIU Xin-yu | School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450001, China |
| WANG Li-guo | School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450001, China |
| REN Chen-xing | School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450001, China |
| CHANG Lei | School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450001, China |
| WANG Jun | School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450001, China |
| GUAN Shao-kang | School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450001, China |
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| 中文摘要: |
| 目的 在医用镁合金骨螺钉表面构建羟基磷灰石涂层，有效控制其降解速率。方法 利用微弧电泳/水热复合方法，在形貌复杂的骨螺钉表面制备涂层。该方法首先利用电解抛光对骨螺钉表面进行表面预处理，采用微弧电泳技术在其表面制备羟基磷灰石涂层，再利用水热合成对微弧电泳涂层进行封孔。利用XRD、SEM、AFM等分析手段对涂层显微结构进行分析，利用体外浸泡实验和电化学实验对涂层耐腐蚀性能及其对钙磷盐的诱导特性进行了评价。结果 在电解抛光电流0.14 A、抛光时间2 min的工艺条件下进行电解抛光预处理，可以提高基体和涂层的结合性能。由于骨螺钉的特殊形状，在微弧电泳电解液中添加丙三醇，并通过调整电解液中丙三醇含量优化微弧电泳工艺（电压155 V，反应时间20 min），能有效抑制尖端放电现象，防止膜层组织疏松和大量的氧化物堆积，以及涂层剥落甚至基体烧蚀的现象。再优化水热合成工艺参数（处理液pH值8.5，反应时间1.5 h，反应温度393 K）对微弧电泳涂层进行封孔，得到微弧电泳/水热复合涂层。结论 微弧电泳/水热复合涂层表面形貌为菜花状结构，由纳米棒状羟基磷灰石组装而成，均匀致密，结晶性好。电化学腐蚀测试表明，制备复合涂层后，骨螺钉的腐蚀电流密度降低了一个数量级。在模拟体液中浸泡6天，骨螺钉的形貌依然完整，说明水热复合涂层在改善生物相容性的同时，提高了骨螺钉的耐腐蚀性能。但微动摩擦磨损测试显示，水热复合封孔处理后磨损性能下降。 |
| 英文摘要: |
| The work aims to control the degradation rate effectively by preparing hydroxyapatite coating on the surface of biomagnesium alloy bone screws. Coating was prepared on the surface of bone screws with complex morphology by means of micro-arc electrophoresis and hydrothermal synthesis. First, electrolytic polishing was used to pretreat the surface of bone screws. Subsequently, amorphous hydroxyapatite coating was prepared on the surface by virtue of micro-arc electrophoresis. Finally, the micro-arc electrodeposition coating was sealed by virtue of hydrothermal synthesis to obtain hydroxyapatite composite coating is with high purity and good crystallinity. Microstructures, morphology and composition of the composite coating were characterized by XRD, SEM, AFM etc. In vitro immersion test and electrochemical experiment were carried out in T. Kokubo's stimulated body fluid (SBF) to evaluate the corrosion resistance and the ability to induce the precipitation of calcium orthophosphates of this composite coating. Electrolytic polishing pretreatment was carried out provided with electrolytic polishing current of 0.14 A and polishing time of 2 min, so as to improve binding strength between the substrate and coating. In the process of micro-arc electrophoresis, serious tip discharge was observed on surface due to its specific shape of the bone screws. The addition of glycerol into the micro-arc electrophoresis electrolyte could effectively restrain the electric discharge phenomena in the tip, and prevent porosity of the film structure, deposition of numerous oxides, exfoliation of the coating and even ablation of the matrix by adjusting the content of glycerol in the electrolyte and optimizing the micro-arc electrophoresis process (voltage of 155 V and reaction time of 20 min). Then the micro-arc electrophoresis coating was sealed by optimizing hydrothermal synthesis parameters (pH 8.5, reaction time of 1.5 h and reaction temperature 393k) to form HA composite coating. The morphology of micro-arc electrophoresis/hydrothermal synthesis composite coating is cauliflower-like structure assembled by hydroxyapatite nano rods. The coating is uniform, compact and of good crystallinity. The electrochemical corrosion test shows that, corrosion current density of the bone screws with the composite coating decreases by one order of magnitude, and morphology of the bone screws is still intact after 6 days of immersion in simulated body fluid, indicating that micro-arc electrophoresis/hydrothermal composite coating could improve biocompatibility to some extent and especially the corrosion resistance. However, the fretting friction-wear test shows that the wear resistance decreases after hydrothermal composite sealing. |
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